EP1004617A1 - Procédé de préparation d'un matériau cellulaire caoutchouteux - Google Patents
Procédé de préparation d'un matériau cellulaire caoutchouteux Download PDFInfo
- Publication number
- EP1004617A1 EP1004617A1 EP99402910A EP99402910A EP1004617A1 EP 1004617 A1 EP1004617 A1 EP 1004617A1 EP 99402910 A EP99402910 A EP 99402910A EP 99402910 A EP99402910 A EP 99402910A EP 1004617 A1 EP1004617 A1 EP 1004617A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- crosslinking
- expansion
- rubbery
- rubber mixture
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2321/00—Characterised by the use of unspecified rubbers
Definitions
- the present invention relates to a process for preparing a expanded rubbery cellular material.
- the present invention relates to the manufacture of rubber materials in the form of a strip or thin sheet composed of at least one layer of rubber or related material, preferably applied on a flexible support and generally made up of a fabric.
- Such articles are used in particular in furniture, especially for the making of carpet backing, in the clothing industry and in particular for the production of shoe soles.
- the processes conventionally used to prepare this type of rubbery cellular material implement a succession operations involving in particular at least one calendering operation and crosslinking.
- calendering refers to a manufacturing technique sheets, plates, or films comprising laminating a material thermoplastic between several cylinders constituting the grille.
- this calendering operation is associated with a coating of the rubbery material on the surface of a porous support, for example a fabric.
- the rubber material is subjected to an operation of vulcanization or crosslinking during which the chemical transformation of the starting elastomeric mixture into a network reticle.
- the present invention relates more particularly to the preparation of so-called expanded rubber articles.
- this agent By decomposing under the action of heat, this agent generates gases, which gases develop bubbles in the medium low viscosity elastomer. The result is an expanded cell structure.
- the first object of the present invention is a process for preparing expanded rubbery cellular material from of an expandable rubber mixture according to which said mixture is subjected at least one calendering, crosslinking and expanding operation characterized in that the crosslinking operation is carried out simultaneously with the expansion operation, continuously and on a horizontal plane and in that said expandable rubber mix has a Mooney number between 40 and 80 estimated at a temperature of about 50 ° C and includes, in addition to at least a rubbery material, at least one crosslinking system and one system expansion, said systems being active at the same temperature included between 150 ° C and 210 ° C.
- these two stages of crosslinking and expansion are carried out continuously by horizontal displacement material just calendered, in an enclosure, preferably a tunnel brought to the appropriate temperature for the concomitant execution of crosslinking and expansion, not in an oven and on a vertical plane in accordance with conventional methods.
- continuous crosslinking and expansion of the calendering operation i.e. without cutting the production line, is particularly interesting on an industrial level.
- the claimed preparation process in the context of the present invention also involves the implementation of an expandable rubber mixture having characteristics specific.
- One of these characteristics relates in particular to the viscosity of this mixture.
- This mixture must have a Mooney index between 40 and 80 estimated at a temperature of around 50 ° C.
- This Mooney consistometric index actually corresponds to a torque value.
- the Mooney consistometric index is therefore the value of the torque of torsion exerted on the rotor, expressed in Mooney units, indicated by the device after a warm-up time of 1 minute followed by a rotation time of the rotor usually 4 to 8 minutes. In the case of the present invention, this index is measured for a temperature of about 50 ° C of the rotor.
- this index is measured for more than precision, please refer to the notice published by the French standard NFT43005 as of December 1991.
- the rubbery or even elastomeric components are so chosen so as to lead to a starting rubber mixture having a Mooney consistometric index in accordance with this invention.
- rubbery material means natural, synthetic rubber or their mixtures.
- the initial mixture includes at least one crosslinking system and one expansion system which are all two active ingredients at the same temperature, between 150 ° C and 210 ° C.
- the system of crosslinking comprises at least one crosslinking agent, also known as an accelerator primary.
- This crosslinking agent preferably belongs to the family of thiazoles, quinones or quinones-dioximes.
- It is preferably present in an amount of 0.5 to 8% by weight per relative to the mass of the rubber material to be transformed.
- This primary accelerator is preferably associated with a agent says secondary accelerator.
- This secondary accelerator preferably belongs to the family metallic or non-metallic dithiocarbamates, xanthates metallic or non-metallic or to the thiazole family.
- This secondary accelerator is generally present at the rate of 0.2 to 2% by weight and more preferably 0.2 to 1.5% relative to the weight of the rubbery material.
- the crosslinking system may be present in the mixture rubbery to transform at a rate of about 4 to 10% by weight relative to the weight of the rubbery material.
- the expansion system includes at least a blowing agent.
- This blowing agent may belong to the family of azodicarbonamides or the sulfohydrazide family.
- the decomposition temperature of blowing agents related to azodicarbonamides varies between 160 and 210 ° C, as for the agents bulbs belonging to the sulfohydrazide family, their temperature of decomposition is greater than 105 ° C.
- blowing agents are generally associated within the expansion system with at least one expansion regulator.
- expansion regulators suitable for the present invention one can more particularly name urea and its derivatives, zinc-based compounds of the zinc oxide, zinc stearate type, as well as amino compounds.
- the expansion system is incorporated correctly from about 2 to 10% by weight of the rubbery material to be treated.
- Cross-linking and expansion reactions are generally performed at atmospheric pressure.
- the rubber compound to transformer can also incorporate other conventional additives such as anti-oxidation agents intended to prevent premature aging of the rubbery mixture.
- charges into it. more or less important proportion. It can be reinforcing fillers like kaolin or carbonate of magnesia or even carbon black. he can also be calcium carbonate or silicate or else silica ultra-fine. The charges are in fact products that can be incorporated into this mixing without lowering its mechanical qualities too much. By way of illustration of others fillers, one can quote the chalk, the kaolin, the sulphate of baryte, the kieselguhr, the talc and lithopone.
- plasticizers oils derived from petroleum such as naphthenic compounds, aromatic and / or aliphatic, the plasticizers of the phthalate family such as dioctyphthalate (DOP) and type flame retardant plasticizers chlorinated phosphates and paraffins.
- DOP dioctyphthalate
- type flame retardant plasticizers chlorinated phosphates and paraffins.
- the rubber mixture may include pigments for coloring the final material, odors for combat odor from vulcanized rubber, abrasives for items that must provide abrasion or polishing work, flame retardants for articles which one wishes to protect as far as possible against fire, hardeners to avoid deformation during certain manufacturing, retarders to sometimes moderate the too rapid action of accelerators, peptizers to soften rubber, etc.
- the operations of crosslinking and expansion are carried out in a time not exceeding 5 minutes. More preferably, they are carried out within an inclusive period between 1 to 3 minutes.
- this residence time at the temperature of crosslinking and expansion can be extended; however insofar as this extension does not bring any additional particular effect, it does not present little industrial interest.
- the operation calendering is also carried out continuously, that is to say so uninterrupted in the manufacturing chain.
- the rubber mixture expandable may, following the calendering operation and beforehand during the crosslinking and expansion operation, undergo a graining operation.
- This operation aims to apply on at least one of the faces of the rubberized cellular material calendered with unevennesses forming protrusions and hollows all of whose surfaces have a certain grain and are more or less regular and not smooth.
- the appearance of the product is considerably improved which is particularly advantageous when said article is intended for decoration.
- the claimed process advantageously leads to materials expanded rubber cells with a regular cell structure which gives a smooth surface appearance.
- the cells are mostly elliptical in shape with the major axis oriented vertically. This elliptical shape as well as the cellular regularity gives the product as well obtained a particularly advantageous elastic recovery.
- the present invention also relates to a method such as defined above characterized in that the expandable rubber mixture is laminated on a strip of fabric and in that said strip scrolls so continuous and on a horizontal plane through an enclosure brought to a temperature between 150 and 210 ° C, its residence time in said enclosure being sufficient for the simultaneous carrying out of the operations of crosslinking and expanding and in that said strip of cellular tissue expanded rubbery thus obtained is recovered at the outlet of said pregnant.
- composition of the rubber mixture to be expanded and crosslinked is as follows: in weight * Natural rubber type SMR CV 100 * Pepticant (dibenzyl amidodiphenyl disulfide) 0.1-0.2 * Dummy 5-15 * Chalk 20-60 * Kaolin 10-30 * Naphthenic plasticizer 30-50 * Paraffin 1-4 * ZnO 5-10 * Stearic acid 1-3 * Protection agents 1-3 * Sulfur 1-2.5 * Zinc diethyl dithiocarbamate 0.3-1.4 * Benzothiazyl disulfide 1-2.5 * Sulfohydrazide blowing agent 4-10 * Urea 4 - 10
- the rubbery mixture is then rolled on a support textile, followed by an anti-sticking treatment.
- the laminated rubber mix is then rolled up.
- the rolls of coated fabric from the grille are then arranged in an unwinding device.
- the coated fabric is unrolled and goes into an accumulator where it can be temporarily stored.
- Downstream of the grille a series brush device is arranged. cleaning device and a gram device for printing an embossed pattern.
- the strip obtained is directed towards an expansion tunnel and crosslinking brought to a temperature of 180 ° C.
- the tape scrolls so continues through this enclosure so that its residence time there not exceed 5 minutes.
- the tunnel exit is cooled and the coated fabric expanded is rolled up.
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- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
Abstract
Description
en poids | |
* Caoutchouc naturel type SMR CV | 100 |
* Peptisant (dibenzyl amidodiphényl disulfure) | 0,1-0,2 |
* Factice | 5-15 |
* Craie | 20-60 |
* Kaolin | 10-30 |
* Plastifiant naphténique | 30-50 |
* Paraffine | 1-4 |
* ZnO | 5-10 |
* Acide stéarique | 1-3 |
* Agents de protection | 1-3 |
* Soufre | 1-2,5 |
* Diéthyl dithiocarbamate de zinc | 0,3-1,4 |
* Disulfure de benzothiazyle | 1-2,5 |
* Agent gonflant type Sulfohydrazide | 4-10 |
* Urée | 4 - 10 |
Claims (20)
- Procédé de préparation d'un matériau cellulaire caoutchouteux expansé à partir d'un mélange caoutchouteux expansible selon lequel ledit mélange est soumis à au moins une opération de calandrage, de réticulation et d'expansion caractérisé en ce que l'opération de réticulation est réalisée simultanément à l'opération d'expansion, en continu et sur un plan horizontal et en ce que ledit mélange caoutchouteux expansible présente un indice Mooney compris entre 40 et 80 estimé à une température d'environ 50°C et comprend, outre au moins un matériau caoutchouteux, au moins un système de réticulation et un système d'expansion, lesdits systèmes étant actifs à une même température comprise entre 150° C et 210° C.
- Procédé selon la revendication 1, caractérisé en ce que les opérations de réticulation et d'expansion sont réalisées en un temps n'excédant pas 5 minutes.
- Procédé selon l'une des revendications 1 à 2, caractérisé en ce que les opérations de réticulation et d'expansion sont réalisées en un temps compris entre environ 1 et 3 minutes.
- Procédé selon l'une des revendications précédentes, caractérisé en ce que l'opération de calandrage est également réalisée en continu.
- Procédé selon l'une des revendications 1 à 4, caractérisé en ce que le mélange caoutchouteux calandré subit préalablement à l'opération de réticulation et d'expansion une opération de grainage.
- Procédé selon l'une des revendications précédentes, caractérisé en ce que le système d'expansion comprend au moins un agent gonflant.
- Procédé selon la revendication 6, caractérisé en ce que l'agent gonflant appartient à la famille des azodicarbonamides ou des sulfohydrazides.
- Procédé selon la revendication 6 ou 7, caractérisé en ce que le système d'expansion comprend en outre un régulateur d'expansion.
- Procédé selon la revendication 8, caractérisé en ce que le régulateur d'expansion est choisi parmi l'urée et ses dérivés, les composés à base de zinc de type oxyde de zinc, stéarate de zinc, ainsi que les composés aminés.
- Procédé selon l'une des revendications précédentes, caractérisé en ce que le système d'expansion est incorporé à raison d'environ 2 à 10 % en poids du mélange caoutchouteux à transformer.
- Procédé selon l'une des revendications précédentes, caractérisé en ce que le système de réticulation comprend au moins un agent réticulant.
- Procédé selon la revendication 11, caractérisé en ce que l'agent réticulant appartient à la famille des thiazoles, des quinones ou quinones-dioximes.
- Procédé selon la revendication 11 ou 12, caractérisé en ce que le système de réticulation comprend, en outre, au moins un accélérateur secondaire.
- Procédé selon la revendication 13 caractérisé en ce que l'accélérateur secondaire appartient à la famille des dithiocarbamates métalliques ou non métalliques, des xanthates métalliques ou non métalliques ou des thiazoles.
- Procédé selon l'une des revendications précédentes, caractérisé en ce que le système de réticulation est présent à raison d'environ 4 à 10 % en poids par rapport au poids du mélange caoutchouteux expansible à traiter.
- Procédé selon l'une des revendications précédentes, caractérisé en ce que le mélange caoutchouteux expansible à traiter comprend en outre un ou plusieurs agents plastifiants.
- Procédé selon l'une des revendications précédentes, caractérisé en ce que les opérations de réticulation et d'expansion sont réalisées à la pression atmosphérique.
- Procédé selon l'une des revendications précédentes, caractérisé en ce que le mélange caoutchouteux est enduit lors de l'opération de calandrage sur un support fibreux.
- Procédé selon la revendication 18, caractérisé en ce que le support fibreux est une bande de tissu.
- Procédé selon la revendication 18 ou 19, caractérisé en ce que le mélange caoutchouteux expansible est laminé sur une bande de tissu et en ce que ladite bande défile de manière continue et sur un plan horizontal à travers une enceinte portée à une température comprise entre 150 °C et 210°C son temps de séjour dans ladite enceinte étant suffisant pour la réalisation simultanée des opérations de réticulation et expansion et en ce que ladite bande de tissu cellulaire caoutchouteux expansée ainsi obtenue est récupérée à la sortie de ladite enceinte.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9814797 | 1998-11-24 | ||
FR9814797A FR2786194B1 (fr) | 1998-11-24 | 1998-11-24 | Procede de preparation d'un materiau cellulaire caoutchouteux expanse |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1004617A1 true EP1004617A1 (fr) | 2000-05-31 |
EP1004617B1 EP1004617B1 (fr) | 2002-01-30 |
Family
ID=9533134
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP99402910A Expired - Lifetime EP1004617B1 (fr) | 1998-11-24 | 1999-11-23 | Procédé de préparation d'un matériau cellulaire caoutchouteux |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP1004617B1 (fr) |
AT (1) | ATE212650T1 (fr) |
DE (1) | DE69900839T2 (fr) |
ES (1) | ES2168839T3 (fr) |
FR (1) | FR2786194B1 (fr) |
PT (1) | PT1004617E (fr) |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1350137A (en) * | 1970-11-09 | 1974-04-18 | Gen Tire & Rubber Co | Pneumatogen for cellular rubber products |
US4252909A (en) * | 1978-03-08 | 1981-02-24 | Mitsui Petrochemical Industries, Ltd. | Free-expandable rubbery composition |
US4983685A (en) * | 1986-06-10 | 1991-01-08 | Sumitomo Chemical Company, Limited | Methods for production of crosslinked rubber products |
-
1998
- 1998-11-24 FR FR9814797A patent/FR2786194B1/fr not_active Expired - Fee Related
-
1999
- 1999-11-23 ES ES99402910T patent/ES2168839T3/es not_active Expired - Lifetime
- 1999-11-23 DE DE69900839T patent/DE69900839T2/de not_active Expired - Fee Related
- 1999-11-23 EP EP99402910A patent/EP1004617B1/fr not_active Expired - Lifetime
- 1999-11-23 AT AT99402910T patent/ATE212650T1/de not_active IP Right Cessation
- 1999-11-23 PT PT99402910T patent/PT1004617E/pt unknown
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1350137A (en) * | 1970-11-09 | 1974-04-18 | Gen Tire & Rubber Co | Pneumatogen for cellular rubber products |
US4252909A (en) * | 1978-03-08 | 1981-02-24 | Mitsui Petrochemical Industries, Ltd. | Free-expandable rubbery composition |
US4983685A (en) * | 1986-06-10 | 1991-01-08 | Sumitomo Chemical Company, Limited | Methods for production of crosslinked rubber products |
Also Published As
Publication number | Publication date |
---|---|
DE69900839T2 (de) | 2002-09-19 |
DE69900839D1 (de) | 2002-03-14 |
EP1004617B1 (fr) | 2002-01-30 |
PT1004617E (pt) | 2002-07-31 |
FR2786194B1 (fr) | 2001-02-09 |
FR2786194A1 (fr) | 2000-05-26 |
ES2168839T3 (es) | 2002-06-16 |
ATE212650T1 (de) | 2002-02-15 |
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